Apparatus for producing ketones



R. R. WILLIAMS AET AL APPARATUS` FOR PRODUCING KETONES Filed Mar. 51, 1919 Apr. 3, 1923.

Patented pr. 3, 1923.

UNITED STATES I 1,450,569 PATENT orties..v

ROBERT R. WILLIAMS, OF CHICAGO, ILLINOIS, AND HERBERT L. J'. HALLER, OF CIN- CINNATI, OHIO, ASSIGNORS, BY MESNE ASSIGNMENTS, TO SETH B. HUNT, TRUSTEE,`

OF MOUNT KISCO, NEW YORK.

APPARATUS FOR PROEUCING KETONES.

/ Application filed March 31, 1919. Serial No. 286,430.

To all whom t may-concern:

Be it known that we, Ronnn'r R. WILLIAMS and HERBERT L, J. HALLER, citizens of the U. S., residing in the city of Chicago, county of Cook, State of Illinois, and in the city of Cincinnati, county of Hamilton, State of Oh'io, respectively, have invented certain new and useful Improvements in an Apparatus for Producing Ketones, of which the following is a full, clear, and exact description.

This invention relates to the production of ketones from secondary alcohols and provides a process and apparatus for such production. The invention relates particularly to a process and apparatus for effecting the continuous conversion of secondary alcohols to ketones b-y catalytic action. tion involves the use of a ,particular catalytic agent, a zinc-copper alloy, or brass.

The process, which may be conducted in the apparatus described and claimed, provides for the mixing of the secondary alcohols to be treated either in the form of vapors or liquid with air or other aeriform oxygen containing medium, the heating of this mixture! and the introduction of this material into contact with the catalytic agent.

The details of the process and apparatus provide for continuous conversion. The apparatus included in the invention will be understood from the attached drawing in which:

Figure 1 is a view, largely diagrammatic, illustrating the relative position Aof the apparatus parts, g

Figure 2 isan enlarged View in cross section illustrating the details of construction of the catalytic reaction chamber. j j

Referring to the details of the drawing, 1 is a still for generating vapors of the secondary alcohols to be treated, and heating means for the still is indicated by the burner 2.

Still 1 and is recurved and'continued as a downwardly extending spiral coil 4. The coil 4 is preferably entirely enclosed within a vertical cylindrical heating jacket 5 which is a pre-heating chamber for the spiral tube 4, as Will'be described. The lower end of Vthe jacket 5 is provided with an annular flange 6. Positioned beneath the heating jacket 5 is a cylindrical member 7 constitutf- The inven- A tube 3 extends from the -top of the of the spiral tube 4 is continued as a straight tube 4a within the reaction chamber 7, positioned centrally thereof, and extending nearly to the lower endg-of the member 7. The details of construction of the member 7, as illustrated in Figure 2, show the outer walls with the closed lowerY end and fthe flange 8. A centrally located tube 10 provided with a short inwardly extending flange 11 at its lower end is spaced from the lower end-of the member 7 by spacing bar 12. An opening 13 isthus provided in the tube 10 between the edges of the flange 11, and a-space 14 is provided between the bar 12 and the lower end of the member 7. In 'the annular space 15 between the walls of the tube 10 and member 7 there is a mass of catalytic material 16, illustrated herein as being woven wire gauze wrapped around the tube 10. Thematerial of this gauze, in accordance with the disclosure of application Serial No. 287,285, filed April 3, 1919, is preferably a zinc copper alloy. rI`he walls of the member-7 should be formed of iron or steel for the sake of strength and durability but preferably arelined with a thin wall of brass or copper, `Zinc alloy, or galvanized with a coat of zinc. lower end 4a of the tube is adapted to extend down intothe tube 10 substantially filling the same and rest upon the flange 11.

The heating jacket 5- is provided at its upper end with a laterally projecting vent pipe 17 extending as a coil through a condenser box 18 and terminating in areceiver 19 which latter is adapted to trap condensed material.. A series of scrubbers 20 are connected to the receiver 19 and are adapted to wash residual gases. A vacuum pump, not shown, is attached to the last scrubber and serves to promote the free llow of material through the apparatus which is thus operated under slightly reduced pressure. Immediately above the heating jacket 5 and connected to the tube 3 is an alcohol intake The straight als ` with the alcohol, and both 3 and 3* are provided with suitable regulating valves. A thermometer is indicated at 5 as serving to indicate the ten'iperature of vapors at a time when they are leaving the catalyst.

In operating the process, the secondary alcohol may be introduced into the tube 3 either as a vapor from the still 1 or as a liquid through the intake pipe 3a. Air is admitted through the pipe 3b and is thoroughly mixed with the alcohol vapors during the passage down through the coil 4- which in turn is heated b-y the hot vapors ascending from the. reaction chamber 7. After the alcohol and air flow is initiated and adjusted so that a small amount of the mixture is admitted to the reaction chamber, external heat is app-lied for five to twenty minutes and until the walls of the chamber 7 show a moderate red hea-t. This heat may be applied by any suitable means such as a blow torch and should be app-lied directly to the exterior of the reaction chamber 7. This heat is continued until the thermometer shows a temperature of about 200O C., then additional amounts of the mixture of alcohol and air is admitted and if the apparatus has been heated suiiiciently white fumes will appear in the receiver 19, and it is thus recognized that the catalytic reaction .is Well started. At the same time the temperature indicated by the thermometer 5a beginsI to rise at an accelerated rate. If these indications of the operation of the catalyst do not occur the ope-rator recognizes that the catalyst was not sufficiently hot to react properly and ltherefore the mixture of alcohol and air is shut ofi' and the exterior application of heat to lthe reaction chamber 7 again made. As/soon as the reaction is proceeding satisfactorily the external heating is stopped and with the proper quantity and proportion of alcohol and air provided the temperature of the reaction chamber is automatically maintained at the desired point. The heat produced by the conversion of the secondary alcohols into ketones by the catalytic action of the mate-rial 16 on the hot mixture of alcohol and air is sufficient to,l

keep the reaction going indefinitely. The hot ketone vapors pass upwardly from the material 16 thro-ugh the heating chamber 5 and there serve to heat the tube 4 and thus pre-heat the air and alcohol prior to contact with the catalyst. The hot vapors then pass out through the pipe 17 and through the condenser box 18 and the liquid ketones are trapped in the receiver 19.

.In the normal operation of the process the temperature of the gases prior to enterlthan the temperature of the material itself.

The gases leave the material 16 and enter 75 the combined outlet pipe and heating jacket 5 at a temperature varying probably from 300O C. to 400 C. and cool off gradually as they rise until at the point where they leave the vicinity of the pre-heating tube 4 and enter the pipe 17 their temperature is usually about 100o C. to 120o C. These temperatures will of course vary according to the size and arrange-ment of the apparatus and the exact nature, quality and purity of the alcohols undergoing treatment. The rate oi admission of the alcohol and air will also cause the above sta-ted condition to vary. Operation of apparatus constructed in accordance with the present description has provided the data given hereinbefore so that these figures of temperatures are representative of actual conditions.

It will be noticed that the process dispenses with any application o-f external heat except for use in starting the reaction. The invention also provides for the utilization of hot vapors to pre-heat fresh material` progressively higher temperatures thus being met as the cool ,untreated material approaches the catalyst. Another novel feature is to be found in the separation of the reaction chamber from the heating chamber by means of an asbestos gasket. It is especially important that no heat be removed from the reaction chamber by direct contact- 4 with any other body, since the convenience of the apparatus depends chieti on selfmaintenance of temperatures. he use of an insulating gasket in the relation indicated with respect to the reaction chamber performs a peculiar function in the present invention.

lVhat we claim is:

1. An apparatus for conducting exothermic gas phase reactions. which comprises a heating chamber through which outgoing 2. An apparatus for conducting exothermic gas phase reactions, which comprises a heating chamber through which outgoing products of reaction must pass, a reaction chamber opening at one end into said heating chamber and closed at its opposite end, an

p open center body of catalytic material in the reaction chamber, a pipe extending through the heating chamber and through the body of catalytic material and having its open end substantially adjacent to the closed end of the reaction chamber, whereby materials incoming through said pipe are heated first by outgoing products of reaction passing backwardly'from the reaction chamber, and then by passing through the catalytic mate- Q rial before being delivered into contact therewith.

3. Apparatus for producin catalytic conversion which apparatus inc udes a heating chamber, a reaction chamber extending beyond said heating chamber and constituting a continuation thereof, a tubular member eX-.

tending through said heating chamber and within said reaction chamber and terminating with one open end within said reaction chamber near the end thereof remote from the heating chamber, means connected to said tubular member at a point outside of said heating chamber for introducing material to be treated, and a catalytic material disposed within said reaction chamber and between the open end of said tubular member and the end of said reaction chamber nearest to the heating chamber.

4. Apparatus for producin catalytic conversion, which apparatus incldes a heating chamber having metal walls, a reaction chamber having metal walls formed separately from and arranged as a continuation of said heating chamber, a catalyticl material within said reaction chamber, and an asbestos gasket between said reaction chamber and said heating chamber, and fastening means holding said reaction chamber and heating chamber in fixed relation to each other.

5. Apparatus for producin catalytic conversion, which apparatus incIudes a heating chamber having metal Walls, a reaction chamber having metalwalls formed separately from and arranged as a continuation of said heating chamber, a catalytic material within said reaction chamber, a gasket of f material of low heat conductivity as compared with the material of the walls of said chambers, and fastening means holding said reaction chamber and said heating chamber in fixed relation to each other,

6. In apparatus for producing conversion of secondary alcohols to ketones, a heating chamber having metal walls, a reaction chamber having metal walls extending beyond said heating chamber'` and forming a continuation thereof, a gasket of low heat conductivity between said chambers, a tubular member for supplying the alcohols and oxygen extending through said heating chamber and into said reaction chamber and opening into the reaction chamber, and a catalytic body of annular form in said reaction chamber and surrounding said tubular member.

7. In apparatus for converting seconda-ry alcohols to ketones, a reaction chamber having metal Walls exposed for application of external heat thereto in starting the reaction, a heating chamber also of metal and attached to the reaction chamber and forming a continuation thereof, a member of low heat conductivity interposed between said chambers, a tubular member for supplying the alcohols and oxygen extending through the heating chamber and nearly through the reaction chamber, and an annular porous spool of metallic catalytic material within the reaction chamber and substantially-filling the space therein about said tubular member.

8. An apparatus for conducting exothermic gas phase reactions, comprising a heating chamber through which outgoing products of the reaction must pass, a reaction chamber having a mass of catalytic material so placedthat gases tobe treated must pass therethrough before entering the heating chamber, and a pipe passing through such heating chamber and the mass'bf catalytic material and of sufficient length so that the heat of reaction will vaporize liquids introduced into such pipe for treatment before the material so introduced enters the reaction chamber.

In testimony whereof witness our signatures.

ROBERT a. WILLIAMS. HERBERT L. J. HALLER. 

